CN104045843B - A kind of preparation method of anti-bacterial hydrogel - Google Patents
A kind of preparation method of anti-bacterial hydrogel Download PDFInfo
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- CN104045843B CN104045843B CN201410302200.2A CN201410302200A CN104045843B CN 104045843 B CN104045843 B CN 104045843B CN 201410302200 A CN201410302200 A CN 201410302200A CN 104045843 B CN104045843 B CN 104045843B
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Abstract
The invention discloses the preparation method of a kind of anti-bacterial hydrogel, comprise the following steps: step 1, utilize oxidant that the activity hydroxy in hemicellulose is oxidized to aldehyde radical, obtain dialdehyde hemicellulose；Step 2, the dialdehyde hemicellulose solution of excess reacts with chitosan solution, forms the mixture that hydrogel is formed with residue dialdehyde hemicellulose；Step 3, immerses silver ion solution by described mixture, makes Argent grain adsorb at hydrogel network body structure surface, makes anti-bacterial hydrogel.Utilize the inventive method, hemicellulose utilizes oxidant modified, gives its functional groups, benefit and the amino generation schiff base reaction in chitosan.The preparation method reaction temperature condition of anti-bacterial hydrogel is low, and energy consumption is little, it is easy to put into commercial production.Additionally, the Argent grain of the anti-bacterial hydrogel absorption prepared reaches Nano grade, there is excellent antibacterial effect.
Description
Technical field
The present invention relates to anti-bacterial hydrogel preparing technical field, particularly relate to a kind of utilization half fine
The method that dimension element prepares anti-bacterial hydrogel.
Background technology
Along with China's industrialization development and the raising day by day of people's living standard, people are to the energy
Consume and the demand of synthetic material increases sharply, and the conventional energy resource such as coal, oil and natural gas
The amount of containing is limited, and petrochemical industry base synthetic material is difficult to be biodegradable, and depends on the mankind for existence
Environment causes severe contamination.Therefore, develop and use cleaning Renewable resource and become primary choosing
Select and inexorable trend.It is all that biomass resource has recyclability, aboundresources and environmental friendliness etc.
Many advantages.Hemicellulose as a kind of biomass resource, nature storage is high, it is renewable to have,
The features such as nontoxic, good biodegradable and biocompatibility, therefore development and utilization half
Cellulose meets Sustainable Development Planning, all has raising resource utilization and minimizing environmental pollution
There is important realistic meaning.
Hemicellulose, due to the shortcoming of himself, such as degradable, difficult separation etc., limits half fine
The comprehensive utilization of dimension element.Hydrogel is that developed recently is rapidly by the important merit of people's extensive concern
Can macromolecular material, its good water suction, water conservation and biocompatibility, agricultural, industry,
Medical field application is quite varied.Silver nano material has broad spectrum antibacterial, is nontoxic and ring
The anti-biotic material that border is friendly, it has also become the focus of biomaterial research in recent years.In prior art
The method not preparing anti-bacterial hydrogel with hemicellulose for raw material, half existed extensively, in a large number
Cellulosic material is difficult to apply to anti-bacterial hydrogel preparation field.
Summary of the invention
The purpose of the present invention is to propose to the preparation method of a kind of anti-bacterial hydrogel, to solve existing skill
The method not preparing anti-bacterial hydrogel with hemicellulose for raw material in art, hemicellulosic material is difficult
To be applied to problem prepared by anti-bacterial hydrogel.
In order to solve above-mentioned technical problem, present invention employs following technical scheme: a kind of antibacterial
The preparation method of hydrogel, comprises the following steps:
Step 1, utilizes oxidant that the activity hydroxy in hemicellulose is oxidized to aldehyde radical, obtains double
Aldehyde hemicellulose；
Step 2, the dialdehyde hemicellulose solution of excess reacts with chitosan solution, forms hydrogel
The mixture formed with residue dialdehyde hemicellulose；
Step 3, immerses silver ion solution by described mixture, makes Argent grain adsorb at hydrogel
Network structure surface, makes anti-bacterial hydrogel.
The preparation method of anti-bacterial hydrogel as above, it is preferable that step 1, by 1～2 weights
Amount part sodium metaperiodate and 2～4 weight portion hemicelluloses add in the water of 5～10 weight portions, stirring
To being completely dissolved, regulation pH value is to neutral, in 37 DEG C of stirred in water bath 6～12h；React
Cheng Hou, is centrifuged mixed liquor, and cleans 3～5 times with water, dries and obtains dialdehyde hemicellulose.
Oxidant is in addition to such as periodate, it is also possible to select bichromate, permanganate, chlorate etc..
The preparation method of anti-bacterial hydrogel as above, it is preferable that step 2, described dialdehyde half
Cellulose solution is mass concentration 5～the dialdehyde hemicellulose aqueous solution of 10%；Described chitosan is molten
Liquid is mass concentration 1～the chitosan acetic acid solution of 5%；Mix described dialdehyde hemicellulose solution and
Chitosan solution, then regulation pH value is to neutral, mixed liquor be placed in 45 DEG C of stirred in water bath 5～
After 10h, it is continuously heating to 90 DEG C of reactions 30～60min, obtains hydrogel after cooling double with residue
The mixture that aldehyde hemicellulose is formed.
The preparation method of anti-bacterial hydrogel as above, it is preferable that step 3, by described mixing
Thing immerses the AgNO that mass concentration is 0.1～5%3In solution, under room temperature, secretly deposit 12～48h, so
After, it is dipped in ammonia spirit removing the AgNO of excess3, finally obtain anti-bacterial hydrogel.
Compared with prior art, the beneficial effects of the present invention is:
1, hemicellulose utilizes oxidant modified, gives its functional groups, benefit and gather with shell
Amino generation schiff base reaction in sugar.
2, the preparation method reaction temperature condition of anti-bacterial hydrogel is low, and energy consumption is little, it is easy to put into work
Industry produces.
The Argent grain of the anti-bacterial hydrogel absorption 3, prepared reaches Nano grade, has excellent
Antibacterial effect.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of anti-bacterial hydrogel prepared by embodiment of the present invention method；
Fig. 2 is the scanning electron microscope (SEM) photograph of anti-bacterial hydrogel prepared by embodiment of the present invention method；
Fig. 3 is the thermal analysis curue of anti-bacterial hydrogel prepared by embodiment of the present invention method；
Fig. 4 is that escherichia coli are suppressed result by anti-bacterial hydrogel prepared by embodiment of the present invention method
Figure；
Fig. 5 is that staphylococcus aureus is pressed down by anti-bacterial hydrogel prepared by embodiment of the present invention method
Result figure processed；
Fig. 6 is the inventive method principle schematic.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail, but not as to this
The restriction of invention.
As shown in Figure 6, in the present invention prepares the method for anti-bacterial hydrogel, hemicellulose molecule
Containing substantial amounts of activity hydroxy on chain, all can be with oxidant generation redox reaction, will half fibre
In dimension element molecule, the hydroxyl oxygen chemical conversion aldehyde radical on C-2 and C-3 position, obtains dialdehyde hemicellulose.
Hemicellulose after oxidation, due to the aldehyde groups with activation, can be sent out with the amino in chitosan
Raw schiff base reaction, meanwhile, can also be formed between hydroxyl hydrogen bond make dialdehyde hemicellulose with
Chitosan forms hydrogel three-dimensional network structure.Being immersed by hydrogel contains in Ag+ solution, excess
Ag+ is reduced by the aldehyde radical in dialdehyde hemicellulose, and Ag nano-particle adsorbs in hydrogel network simultaneously
Network body structure surface.
Embodiment 1
The first step, adds in 10ml water by 1g sodium metaperiodate and 2g hemicellulose, and stirring is to complete
CL, adds NaOH solution regulation pH value the most neutral, 37 DEG C of stirred in water bath 12h.
After having reacted, mixed liquor is centrifuged, and cleans 3 times with water, dry and obtain dialdehyde half fiber
Element；
Second step, 1g chitosan is dissolved in the acetic acid solution of 2v/v%, and stirring is until the most molten
Solve, obtain the chitosan solution of 5wt%；
3rd step, is dissolved in the water 1g dialdehyde hemicellulose, stir, centrifugal after obtain 5wt%
Dialdehyde hemicellulose suspension；
4th step, after being mixed with chitosan solution by dialdehyde hemicellulose solution, regulation pH value is extremely
Neutrality, after mixed liquor is placed in 45 DEG C of stirred in water bath 10h, is continuously heating to 90 DEG C of reaction 60min,
The mixture that hydrogel is formed is obtained with residue dialdehyde hemicellulose after cooling；
5th step, immerses the AgNO of 2wt% by mixture3In solution, secretly deposit 24h under room temperature, so
After, it is dipped in ammonia spirit removing the AgNO of excess3, finally obtain anti-bacterial hydrogel.
As depicted in figs. 1 and 2, finding out through SEM figure, Ag granular size is about 150～250nm
Between, reach Nano grade.In terms of entirety, Ag nano-particle is cubic type, and uniformly
It is distributed in hydrogel network.As it is shown on figure 3, it can be seen that work as temperature from TGA result
When reaching 256.48 DEG C, hydrogel starts to decompose, when temperature reaches 500 DEG C, hydrogel
Decompose and reach 50%.The better heat stability of hydrogel as can be seen here.
Bacteriostatic experiment step: by 10g tryptone, 5g yeast extract, 10gNaCl chlorination
Sodium and 15g agar add container, add deionized water to 1L, and stir preparation culture medium.
Subpackage, in 18cm test tube and conical flask, seals rear 121 degrees Celsius of sterilizing 30min.Take the photograph 4
The strain inclined plane that family name's degree preserves takes out, and sterile working is inoculated in 3 medium slant.After
Slant tube is placed in 37 degree of constant incubators and cultivates 12h.1g hydrogel sterilized water dilutes 100
Times, it is stained with diluent with filter paper and prepares hydrogel thin slice, ultraviolet sterilization 15min.Draw 100
μ L bacteria suspension joins in culture medium, mixing all with after, be quickly poured on one layer well prepared in advance
On culture medium flat plate, put into hydrogel thin slice after solidification, then pour third layer culture medium into.By institute
There is flat board to be placed in and 4 degrees Celsius of refrigerators preserve overnight, next day all flat boards are transferred to 37 degree of perseverances
In temperature incubator, observation of taking pictures after cultivating 24 hours.
Bacteriostatic experiment result: as shown in Figure 4 and Figure 5, hydrogel is to escherichia coli and golden yellow
Staphylococcus has fungistatic effect, has preferably anti-microbial property.
Embodiment 2
The first step, adds in 10ml water by 1g sodium metaperiodate and 2g hemicellulose, and stirring is to complete
CL, adds NaOH solution regulation pH value the most neutral, 37 DEG C of stirred in water bath 12h.
After having reacted, mixed liquor is centrifuged, and cleans 3 times with water, dry and obtain dialdehyde half fiber
Element；
Second step, 0.5g chitosan is dissolved in the acetic acid solution of 1v/v%, and stirring is until completely
Dissolve, obtain the chitosan solution of 2wt%；
3rd step, is dissolved in the water 2g dialdehyde hemicellulose, stir, centrifugal after obtain 10wt%
Dialdehyde hemicellulose suspension；
4th step, after being mixed with chitosan solution by dialdehyde hemicellulose solution, regulation pH value is extremely
Neutrality, after mixed liquor is placed in 45 DEG C of stirred in water bath 10h, is continuously heating to 90 DEG C of reaction 60min,
The mixture that hydrogel is formed is obtained with residue dialdehyde hemicellulose after cooling；
5th step, immerses the AgNO of 2wt% by mixture3In solution, secretly deposit 24h under room temperature, so
After, it is dipped in ammonia spirit removing the AgNO of excess3, finally obtain anti-bacterial hydrogel.
Bacteriostatic experiment result: hydrogel has antibacterial effect to escherichia coli and staphylococcus aureus
Really, there is preferably anti-microbial property.
Above example is only the exemplary embodiment of the present invention, is not used in the restriction present invention, this
The protection domain of invention is defined by the claims.Those skilled in the art can be the present invention's
In essence and protection domain, the present invention is made various amendment or equivalent, this amendment or
Equivalent also should be regarded as being within the scope of the present invention.
Claims (4)
1. the preparation method of an anti-bacterial hydrogel, it is characterised in that comprise the following steps:
Step 1, utilizes oxidant that the activity hydroxy in hemicellulose is oxidized to aldehyde radical, obtains double
Aldehyde hemicellulose；
Step 2, the dialdehyde hemicellulose solution of excess reacts with chitosan solution, forms hydrogel
The mixture formed with residue dialdehyde hemicellulose；
Step 3, immerses silver ion solution by described mixture, makes Argent grain adsorb at hydrogel
Network structure surface, makes anti-bacterial hydrogel.
The preparation method of anti-bacterial hydrogel the most according to claim 1, it is characterised in that
1～2 weight portion sodium metaperiodates and 2～4 weight portion hemicelluloses are added 5～10 weights by step 1
In the water of amount part, stirring is to being completely dissolved, and regulation pH value is to neutral, 37 DEG C of stirred in water bath
6～12h；After having reacted, being centrifuged by mixed liquor, and clean 3～5 times with water, drying obtains
Dialdehyde hemicellulose.
The preparation method of anti-bacterial hydrogel the most according to claim 1 and 2, its feature exists
In, step 2, described dialdehyde hemicellulose solution is mass concentration 5～dialdehyde half fiber of 10%
Element aqueous solution；Described chitosan solution is mass concentration 1～the chitosan acetic acid solution of 5%；Mixing
Described dialdehyde hemicellulose solution and chitosan solution, then regulation pH value is to neutral, mixed liquor
After being placed in 45 DEG C of stirred in water bath 5～10h, it is continuously heating to 90 DEG C of reactions 30～60min, cold
Obtain the mixture that hydrogel is formed with residue dialdehyde hemicellulose the most afterwards.
The preparation method of anti-bacterial hydrogel the most according to claim 3, it is characterised in that
Step 3, by the AgNO that described mixture immersion mass concentration is 0.1～5%3In solution, room temperature
Under secretly deposit 12～48h, remove the AgNO of excess3, finally obtain anti-bacterial hydrogel.
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| CN111410753A (en) * | 2020-03-27 | 2020-07-14 | 西南大学 | Novel chitosan hydrogel and preparation method and application thereof |
| CN112494716A (en) * | 2021-01-15 | 2021-03-16 | 王忠良 | Bacteriostatic hemostatic hydrogel and preparation method thereof |
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| CN113501886B (en) * | 2021-08-17 | 2022-06-21 | 中南大学 | Cellulose nano-silver composite material and preparation method and application thereof |
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| CN101209354B (en) * | 2007-12-25 | 2010-06-02 | 青岛博益特生物材料有限公司 | Medical blood-stopping healing agent for wound-surface and uses thereof |
| CN101463145A (en) * | 2009-01-12 | 2009-06-24 | 武汉理工大学 | Carboxymethyl chitosan / oxidized sodium alginate self-crosslinking antibacterial hydrogel material |
| CN102321271B (en) * | 2011-09-15 | 2012-09-05 | 西安交通大学 | Preparation method for chitosan-based porous scaffolds with biological activity |
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